固相萃取-液相色谱-串联质谱法测定鸡蛋中小檗碱残留量

Determination of berberine residues in eggs by solid phase extraction coupled with liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  鸡蛋  小檗碱  残留量

英文关键词:liquid chromatography-tandem mass spectrometric  egg  berberine  residues

中文摘要:

      目的 建立固相萃取-液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS) 测定鸡蛋中小檗碱残留量的检测方法。方法 样品经80%(V/V)乙腈溶液提取, 经过混合阳离子(mixed-mode, strong cation-exchange, MCX)固相萃取柱净化。采用0.1%甲酸(V/V)-甲醇溶液(A)和0.1%甲酸 -5 mmol/L乙酸铵溶液(B)进行梯度洗脱, 采用正离子模式, 多反应监测, 基质匹配外标法定量分析。结果 小檗碱进样浓度在2~100 ng/mL范围内与峰面积呈良好的线性关系(r2=0.999); 方法检出限和定量限分别为0.5和1.0 μg/kg; 在1.0、2.0、10.0 μg/kg 3个添加水平下, 回收率在62.2%~108.3%之间, 相对标准偏差为5.6%~9.8% (n=6)。结论 本方法简便、准确、快速、灵敏, 适用于鸡蛋中小檗碱残留量的检测。

英文摘要:

      Objective To establish a method for determination of berberine in eggs by solid phase extraction coupled with liquid chromatography-tandem mass spectrometric (LC–MS/MS). Methods Eggs samples were extracted with 80% (V/V) acetonitrile solution and then the extracts were purified by the MCX (mixed-mode, strong cation-exchange) solid phase extraction. The gradient elution was carried out with 0.1% (V/V) formic acid methanol (A) and 0.1% formic acid-5 mmol/L ammonium acetate solution(B). Electrospray positive ion source (ESI+), multiple reaction monitoring (MRM) mode and the matrix-matching external standard method were applied for quantitative analysis. Results There was a good linear correlation between the peak areas and the concentrations of berberine at the range of 2.0–100 ng/mL (r2=0.999), the limit of detection and limit of quantification was 0.5 and 1.0 μg/kg. The recovery rates were 62.2%–108.3% and the relative standard deviations were 5.6%–9.8% at the addition levels of 1.0, 2.0 and 10.0 μg/kg (n=6). Conclusion This method is simple, accurate, fast and sensitive and is suitable for determination of berberine residues in eggs.